Apparatus for treating plastic material



March Z, 1943.1 F. G. GRONEMEYER APPARATUS FOR TREATING PLASTIC MATERIAL Filed Aug. 2, 1940 2 Sheets-Sheet 1 NW NW MN N \w ww MM ww Q Q NQxIN v USN YINVENTOR a 7 4. M

ATTORNEY I Mar ch 1943. H F. e. GRONEMEYER I ,312,

APPARATUS FOR TREATING PLASTIC MATERIAL Filed Aug. 2 1940 2 Sheets-Sheet 2 lN V NTOR 7m! W Y A ay/mp1. {0.90 R) j ATTORNEY Patented Mar. 2, 1943 UNITED STATES TENT OFFICE APPARATUS FOR TREATING PLASTIC Fred G. Gronemeyen Longmeadow, Mass, assignor to Monsanto Chemical Company, St. Louis, Ma, a corporation of Delaware Application August 2, 1940, Serial No. 349,415

quently necessary to dissolve such materials in a suitable solvent. However, such materials, particularly, when they are obtained in the form of substantially large masses, are frequently extremely slow in dissolving, a difiiculty that is generally believed to be related to their high molecular weight. When these materials are brittle and can be ground to a powder soas to increase their rate of solution by increasing their exposed surface, the difliculty of dissolving such materials is reduced. However, when such ma= terials are substantially free from brittleness and, particularly, when they tend to possess such characteristics as flexibility, toughness, gumminess, elasticity, tackiness, adhesiveness and the like, grinding these materials is difiicult, if not impossible, and a serious problem is presented.

For example, high molecular weight masses comprising such plastic materials as polyvinyl acetate have been found to be extremely dificult to dissolve and, thus, have presented a serious problem in the art. One cause of thi difliculty lies in the self-adhesive properties of such materials which makes diificult contact of solvent with large surface areas of the plastic by customary methods of preparing solutions.

One object of this invention i to provide an apparatus whereby plastic materials may be more readily dissolved. Another object is to provide a method and apparatus whereby diiilcultly soluble plastic materials may be rendered more readily soluble. A further object of the present invention is to provide for thev relatively rapid absorption of solvent by self-adhesive plastic materials.

According to the principles of the present invention, it has been found. that extrusion of plastic materials, in such a manner that the plastic mass is repeatedly broken up in the presence of solvent and, preferably, at a raised temperature, transforms such materials initially into plastic-solvent mixtures that can be more readily dissolved and finally into solutions of any desired.

viscosity. In carrying out the process of this invention, it is preferable, in some instancesfto regulate the amount of solvent and other processing conditions so that the plastic material is transformed into a relatively easily soluble plastic-solvent mixture rather than to a complete and readily fiowable solution. While the exact physical condition of the various types of plastic materials may not necessarily be the same at this point, nevertheless, absorption of substantial amounts of solvent by the plastic'will have taken place so that final solution by customary methods of preparing solutions is rendered-easier. The solvent employed in carrying out this process is not l limited to any particular type of solvent and may comprise mixtures of one or more solvents and, if desired, a portion of the solvent may be replaced by a diluent which is a non-solvent for the plastic.

The following is a description of the operation of one embodiment of this invention whereby plastic materials are rendered more readily soluble. Plastic material, at a suitable temperature,

is forced by suitable means, for example, by a rotatably movable feed screw, through a series of -chambers which may be described as mixing chambers. According to this invention, the plastic mass flowing through this series of chambers is formed into one or more section of reduced cross-section at several successive points, by partially blocking the passage of the plastic in a suitable manner, as for example, by employing perforated plates containing a plurality of relatively small openings, hereinafter described as breaker plates, as theend walls of these cham-' bers. Following one. or more of these points of divisionsof the plastic mass, a solvent for the plastic is forced into one or more of these mixing chambers. Thus, during the flow of the plastic through subsequent mixing chambers,

solvent acts on the plastic, said action being enhanced by the increase in exposed surface that occurs as a result of the separation of sections of the mass as the plastic passes through the restricted openings. The points of injection of solvent into the mixing chambers are preferably situated so as to. injection solvent around the plastic material before the separated sections of the plastic mass can re-coalesce, thus enabling the solvent to immediately contact as much of the exposed surface of the plastic mass as possible. In addition, it is particularly preferable that the first injection of solvent follow the first breaker plate in order to immediately start the action of the solvent on the plastic material. If desired,

the mixing chambers may be heated by suitable means to maintain the. plastic at any desired ranged as regards the sizeand number of mixing chambers, the configuration of and the number showing the design of breaker plate.

novel process is shownin the accompanying drawings.

Fig. 1 is a side elevational view of the apparatus embodying the mixing chambers of this invention.

F18. 2 is a sectional view taken on line l-l of Fig. 1 with the solvent pipe shown diagram matically.

Fig. 3 is a sectional view, partly broken away, taken on line 2-2 of Fig. 2 with the solvent 'pipe shown diagrammatically.

Fig. 415 an end view of a breaker plate.

Fig. 5 is a sectional view taken bu line Fig. 4.

Fig. 6 is an enlargement of a portion of Fig. 5 one of the openings in a a--; or

Before explaining in detail the apparatu of the present invention, it is to be understood that the invention is not limitedin its application to the details of construction and arrangement of parts illustrated in the accompanying drawings, since the invention is capable of other embodiments and of being. practised or carried out in various ways. Also, it is to be understood that the phraseology or terminology employed herein is for the P rpose. of description and not of limitation.

The apparatus illustrated in the accompanying drawings comprises a series of hollow casings II, ll, 12 and 13 having cylindrical chambers 36 31, 38 and 39. Attached to casing ill is another hollow casing M, of which only a portion is shown, having cylindrical chamber 40 through which plastic material is supplied to the series of chambers 36, 31, l8 and I! by means of screw I 5. Attached to casing i3 is a hollow tapered connection I 5, through which the processed plastic material is discharged after passage through the series of chambers 36, 31, $8 and 39.'

Chambers 88, 31, 38 and 39 have as end walls, breaker plates l1, l8, I9, 20, and 2|. The series of casings ll, ll, ll, l2 and I3 and discharge connection 16 are fastened together by means of threaded bolts 22 passing through openingsin flanges 23 and tightened by threaded nuts 24 screwed on bolts 22. Gasket material, notshown in the drawings, is situated on both sides of the breaker plates, to prevent leakage of material from the apparatus. 7

bottom of the chamber and re-coalesce.

can be circulated, embracing chambers 36, 31, 38 and 39. Nipples and 4| represent inlet and outlet connections for supplying heating fluids, as for example, steam.

In the operation -of the present invention plastic material, generally in a heated state, is forced by screw I5 from chamber through breaker plate 11 into chamber 36.; The extruded material, which may be in the form of rods, is met, as it enters chamber 36, by solventfrom pipe'25 forced out of openings 29. The solvent tends to prevent theplastic material from recoalescing and, at the same time, begins to soften and dissolve the plastic material. The mixture of plastic material and solvent is continuously forced forward by screw l5 and passes successively through breaker plate i8, chamber 31,

breaker plate 19, chamber 38, breaker plate 20, chamber 39 and finally breaker plate 2| into the discharge connection It. All the chambers 36,'

by extrusion through the first breaker plate cor-' respond in shape to the configurations of the openings in this breaker plate. However, the extruded sections of the plastic are not believed to continue as straight extensions ofzthe conflgurations imparted by the breaker plate openings. In the first place, the plastic material is likely to be substantially soft and, therefore, theinitially extruded sections are liable to sag to the Furthermore, the pressure required to force the plastic through the openings in the succeeding breaker plate tends to hold back plastic material,

Thus, the first mixing chamber tends'to fill up with plastic so that the extruded sections become subject to a great 'Solvent is admitted through pipe "held in position by flange 28 and threaded bolts 21. Openings 29 allow the solvent to flow out of pipe 25 into chamber '36. Shoulder on cap 80 on the end of pipe 25 prevents plastic material from obstructing openings 29.

The breaker plates I1, l8, l9, "and 2! are perforated by circular holes 3|. These circular holes 31 are smaller in size in plate 18 than in plate l1 and smaller in plate 19 than in plate N. The holes in plates 20 and 2| are equal in size but smaller than those in plate ii. The holes 3| in these breaker plates have rounded corners 32 on the side at which the plastic material passes through the breaker plate as shown in Figure 6.

Nipples 33 are provided for attaching pressure auges to chambers 38 and ill. Casings III, ll, 12 and I! are provided with heating means here shown as Jackets 34, through which hot fluids amount of distorting pressure. In addition, the dissolving and softening action of the solvent injected into this chamber contributes to dis.- tortion of the extruded material. Initial extrusion through the succeeding breaker plate forms the plastic material, to some extent, to configurations corresponding to the shapes of the openings in this breaker plate, although previous penetration of solvent may be such as to prevent complete continuity of the extruded material. In addition, the extruded material is subject to the same distorting forces as in the previous chamber. In any event, this second breaker plate is believed to break up the plastic so as to expose fresh surface to the action of the solvent that is moving along with the plastic material. This process of mixing solvent and plastic followed by breaking up the material so as to exposefresh surface to the action of the solvent, is repeated in the succeeding chambers and by the succeeding breaker plates respectively. As the breaker plate openings become smaller, the extruded sections become smaller in cross-sectional area with correspondingly more surface exposed to the solvent. Furthermore, as stated above. the plastic may, in some cases possess less and less continuity as a result of the continued action of The present invention, as previously indicated, 'is applicable to plastic materials broadly.

In general, this invention is particularly valuable for dissolving masses of thermoplastic materials,

as for example, polyvinyl esters. If the process of this invention be employed for dissolving thermosetting resins, it is obvious to those skilled in the art that heating such resins to the insoluble, infusible stage must be avoided. Furthermore, this invention may also be employed in dissolving or partially dissolving plastic materials that are already subdivided or are capable of being sub divided without re-coalescing. In such cases, the utility of the present inventionlis lessened in that an alternative method is more readily available, whereas the solution of tough adhesive plastic masses by customary methods tends to be cumbersome and expensive. Thus, the process and apparatus of this invention are applicable to all soluble materials and mixtures thereof that soften and flow under pressure at temperatures below their decomposition temperatures.

The following is a specific example illustrating the preferred process of the present invention as applied to one type of plastic material. Thepart; are parts by weight in this example.

comprising small masses of polyvinyl acetate substantially unaffected by solvent surrounded by material varying from a readily flowable solution of polyvinyl acetate in ethanol to transparent, jelly-like material comprising polyvinyl actate which had absorbed suflicient solvent to be greatly softened but not sufficient to become a readily fiowable solution. This polyvinyl ace- 1870 parts of vinyl acetate, dissolved in 1430 parts of benzene were polymerized for substantially 4 hours at substantially 74 C. in a suitable reaction vessel. After removal of the benzene by a suitable method, as for example, by steam distillation, a tough, gummy, adhesive mass of polyvinyl acetate was obtained that contained substantially 14 per cent water and was found to possess a viscosity after suitable purification, of substantially 60 centipoises at 20 C.

in a 1 molar solution in benzene. Steam under a pressure of substantially 100 pounds per square inch was then injected into the reaction vessel above the mass of resinous material and the resin was thereby simultaneously heated and forced through a connecting passage into a suitable extruder, for example, a screw feed extruder. Then, the resin was forced by said extruder through the apparatus shown in the accompanying drawings. The pressure exerted on the plastic material was raised by the extruder to substantially 300 pounds per square inch as measured by the pressure gauge situated before the first breaker plate. During passage of the plastic through the mixing chambers, the pressure dropped somewhat and beyond the last breaker plate had droppedto substantially 200 pounds per square inch. The temperature of the plastic was maintained at substantially 110 C. during its passage through the mixing chambers by injecting steam into the jackets around the mixing chambers. A suitable solvent, as for example, e hanol, was injected into the mixing chamber beyond the first breaker plate at such a rate that 2 pounds of ethanol per pound of polyvinyl acetate were admitted at this point. After passingthrough the mixing chambers under the aforesaid conditions, the polyvinyl acetate and ethanol had formed a heterogeneous mixture tate-ethanol mixture was in such a condition that it could now be relatively easily dissolved 4 in any suitable solvent, as for example, ethanol,

or could be pumped through a pipe line for further processing.

It-is obvious that there are numerous'features in the process and preferred apparatus for carrying out the process of the present invention that are subject to wide variation without departing from the essence of the invention.v Among such variables are the following: pressure exerted on the plastic material during extrusion through the mixing chambers, temperature of the plastic material during extrusion; construction and number of mixing chambers; construction of the breaker plates, including the number, size and position of the openings in said breaker plates, number and location of points of injection of solvent into the mixing chambers; amount of solvent injected into the mixing chambers and type of solvent employed.

In the case of polyvinyl acetate, for example such solvents as methanol, acetic acid, a mixture of acetic acid and aqueous formaldehyde, butyl alcohol, butyl acetate and the like may be substituted for the ethanol given in the specific example. i 1

This invention is limited solely by the claims attached hereto.

What is claimed: I

1. In an apparatus for treating .a plastic material with a solvent, a series of intercommunicating chambers separated by perforated plates, means for forcing plastic materialthrough said chambers and perforated plates, meansfor introducing solvent into one of said chambers, said means comprising a conduit extendinginto said chamber in the direction against the flow I of said material and having outlets thereon at a position behind and adjacent the middle of the discharge side of the perforated plate on the inlet side of said chamber, and adapted to direct said solvent, radially from said conduit-- into said. chamber and substantially normaltto the main direction of flow of material through said chamber, and a deflector adapted to prevent plastic material from clogging said outlets on said conduit.

2. An apparatus as defined in claim 1 in which the perforations in said plates are smaller in the direction of flow of plastic material.

3. In an apparatus for treating a plastic material with a solvent, a series of intercommunicating connected chambers, means for forcing plastic material through said chambers under pressure, means for forming said plastic material into a plurality of elongated masses on passing from a first chamber to a second chamber and means for introducing solvent to said second chamber to a location in said second chambar near said last-mentioned means.

4. In an apparatus for treating plastic material with a treating agent, means for formi a separated portions from a mass of plastic mate-- rial, means ,for introducing treating agent to and contacting said exposed surfaces of said portions therewith after forming said separated portions, and means spaced from said first and second mentioned means for intermixing and separated portions and treating agent. I

5. In an apparatus for treating a plastic ma rial with a treating agent, a series of intercom- 'municating chambers, means for forcing plastic plastic material on passing from a first chamber to a subsequent chamber in said series, means sequent chamber near said last mentioned means after formation of said increased surface area termixing said plastic and before recoalescence, and means spaced from said second and third mentioned means for inm'aterial and treating agent.-

FRED G. GRONEMEYER. 

